CN1775849A - Method for preparing high-temperature-rusistance water-expansible rubber - Google Patents
Method for preparing high-temperature-rusistance water-expansible rubber Download PDFInfo
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- CN1775849A CN1775849A CN 200510019972 CN200510019972A CN1775849A CN 1775849 A CN1775849 A CN 1775849A CN 200510019972 CN200510019972 CN 200510019972 CN 200510019972 A CN200510019972 A CN 200510019972A CN 1775849 A CN1775849 A CN 1775849A
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Abstract
The invention relates to a method to manufacture functional rubber that could be expand when meet water between the temperature 25 degree centigrade and 150 degree centigrade. The process is: taking copolymerization by acrylic acid, sodium acrylate, acrylamide, heat endurable modification monomer and cross linking agent to gain heat endurable water absorbing resin powder, then, mixing and vulcanizing the mixture of the powder and rubber to gain high temperature endurable water expanding rubber. It has simple technology and low cost.
Description
Technical field
The present invention relates to the sealing material field, particularly a kind of preparation method of high-temperature-rusistance water-expansible rubber.
Background technology
Hydro-expansive rubber (Water swelling Rubber is called for short WSR) is a kind of new-type functional material, and it is upward introduced wetting ability functional group or hydrophilic component at traditional elastic matrix (rubber) and makes.Its mechanism of action is: when contacting with water, water molecules can be by diffusion, physical action such as capillary and surface adsorption enters in the WSR, and then form extremely strong avidity with hydrophilic radical in the rubber, because hydroaropic substance constantly absorbs moisture, cause rubber generation deformation, when anti deformational force and permeable pressure head reach balance, WSR keeps relative stability, and reaches elasticity and with the effect of water sealing.Since coming out beginning of the eighties late 1970s, WSR is with the dual sealing characteristic of its unique resilient seal sealing and water-swelling sealing.More and more be subject to people's attention.
The water-expansible rubber of holding back with the blending method preparation only just has good water absorbing properties under lower temperature, when temperature during greater than 30 ℃, the water-intake rate of hydro-expansive rubber reduces along with the rising of temperature, when temperature during near 70 ℃, water-swelling hardly, thereby greatly reduce the rate of expansion of hydro-expansive rubber, cause hydro-expansive rubber under high-temperature condition, to expand hardly, do not reach the sealing effect, to such an extent as to be difficult to come into operation, if can carry out modification to water-absorbing resin, make it under hot conditions, have stable structure and high-hydroscopicity energy, thereby widen its use range, for example improve and at high temperature have the water-swellable performance with significant with its hydro-expansive rubber of making as main raw material.
Zhang Yuhong, He Peixin etc. have studied the elastomeric temperature effect of CPE/P (AA-AM) water-swelling, and when temperature during greater than 30 ℃, the water-intake rate of hydro-expansive rubber reduces along with the rising of temperature, when temperature during near 70 ℃, and water-swelling hardly.
Summary of the invention
The objective of the invention is deficiencies such as heat resistance difference at existing hydro-expansive rubber existence, utilize the special monomer of structure as comonomer, preparing high temperature resistant water-absorbing resin, is feedstock production all has the water-swellable performance from 25 ℃ to 150 ℃ high temperature rubber by the physical blending technology with high temperature resistant water-absorbing resin and rubber.The characteristics of this method are: 1. hydro-expansive rubber broad application temperature range, all can use in 25 ℃ to 150 ℃ the temperature range; 2. prepare water-absorbing resin by simple inverse suspension polymerization method, make it then and the rubber physical blending is compound can obtain, this method technology is simple, and equipment requirements is low; 3. can control the water-swelling multiplying power by the proportioning that changes water-absorbing resin and rubber, thereby expansion multiplying power is controlled.
The objective of the invention is to adopt following technical measures to realize:
With mass ratio is vinylformic acid, sodium acrylate, acrylamide, heat resist modification monomer and the linking agent of 20-40: 30-60: 10-50: 10-60: 0.1-10, add in the reactor with 30-100mL solvent and 0.1-5 gram dispersion agent, constantly stir the back of heating up and drip the initiator copolyreaction, filter, methanol wash dry granularity less than the water-absorbing resin powder of 5 μ m, then with water-absorbing resin powder and rubber carry out blend in the mill, add vulcanizing ingredient vulcanize in 25 ℃ to 150 ℃ scopes, all have the water-swellable function rubber.
Described heat resist modification monomer is a vinyl-acetic ester, butyl acrylate, Octyl acrylate, vinylformic acid lauryl alcohol ester, vinylformic acid stearyl alcohol ester, butyl methacrylate, Octyl methacrylate, methacrylic acid lauryl alcohol ester, methacrylic acid stearyl alcohol ester, 2-acrylamido-2-methyl propane sulfonic acid (AMPS), 3-acrylamido oxypropyl trimethyl ammonium chloride, methacryloyl amido oxypropyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride or 2-methylacryoyloxyethyl-dimethyl dodecyl bromination ammonium.
Described linking agent is ethylene glycol diacrylate, Diethylene Glycol double methacrylate, polyoxyethylene glycol double methacrylate, N, N '-methylene-bisacrylamide, tetramethylolmethane double methacrylate or Vinylstyrene.
Described solvent is toluene, dimethylbenzene or hexanaphthene.
Described dispersion agent is span-80, Si Ban-60, Si Ban-20, tween-80, Tween-60, tween 20, Sodium dodecylbenzene sulfonate.
Described rubber is natural rubber, chloroprene rubber, ethylene-propylene rubber(EPR), paracril, chlorinatedpolyethylene, urethanes, viton, silicon rubber, isoprene-isobutylene rubber or styrene-butadiene rubber(SBR).
Described initiator is Potassium Persulphate or ammonium persulphate.
The present invention has following advantage: the particle diameter of (1) high temperature resistant water-absorbing resin is less, less than 5 μ m; (2) hydro-expansive rubber broad application temperature range, 25 ℃ to 150 ℃ high temperature all can use; (3) prepare by simple inverse suspension polymerization method that water-absorbing material makes it then and the rubber physical blending is compound can obtain this material, technology is simple, and equipment requirements is low; (4) can control the water-swelling multiplying power by the proportioning that changes water-absorbing resin and rubber, thereby expansion multiplying power is controlled.
Adopt the hydro-expansive rubber of the present invention's preparation at high temperature to have good water-swellable performance (seeing the following form) than common hydro-expansive rubber.Accurately take by weighing a certain amount of high-temperature-rusistance water-expansible rubber and place the minitype high voltage still, add 5-20 deionized water doubly, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, carries out weighing.
The weight water-intake rate S of hydro-expansive rubber
WCalculate as follows:
W in the formula
1, W
2Be respectively the weight of sample suction front and back.
Relevant water-swellable experimental result
| Sample type (150 ℃, the treatment time: 3day) | Water-swellable multiplying power/% |
| Common hydro-expansive rubber sample of the present invention | 50 400 |
Embodiment
Embodiment 1
With 2 gram vinylformic acid, 4 gram sodium acrylates, 2 gram acrylamides, 2 gram 2-acrylamido-2-methyl propane sulfonic acids, 0.2 gram Diethylene Glycol double methacrylate, 50ml toluene and 1 gram span-80 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the initiator potassium persulfate copolyreaction after 3 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of paracrils, 30 parts of water-absorbing resin powders, 5 parts of zinc oxide, 2 parts of sulphur, 1 part of anti-aging agent, 20 parts of carbon blacks, 2.5 parts of promotor are carried out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 42 grams.
Embodiment 2
With 2.5 gram vinylformic acid, 3 gram sodium acrylates, 3 gram acrylamides, 1.5 gram 3-acrylamido oxypropyl trimethyl ammonium chloride (APTAC), 0.1 gram N, N '-methylene-bisacrylamide, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, be warming up to 60 ℃ under constantly stirring, drip the initiator potassium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of paracrils, 30 parts of water-absorbing resin powders, 5 parts of zinc oxide, 2 parts of sulphur, 1 part of anti-aging agent, 20 parts of carbon blacks, 2.5 parts of promotor are carried out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 43 grams.
Embodiment 3
With 3 gram vinylformic acid, 3.5 gram sodium acrylate, 1.5 gram acrylamide, 2 gram methacryloyl amido oxypropyl trimethyl ammonium chlorides (MPTMA), 0.3 gram N, N '-methylene-bisacrylamide, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, are warming up to 85 ℃ under constantly stirring, and drip the initiator ammonium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash, then with 100 parts of chloroprene rubbers, 30 parts of water-absorbing resin powders, 1 part of stearic acid, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 30 parts of potter's clay carry out blend in mill, vulcanize to such an extent that in 25 ℃ to 150 ℃ scopes, can hold back water swellable rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 39 grams.
Embodiment 4
With 3 gram vinylformic acid, 3 gram sodium acrylates, 3 gram acrylamides, 1 gram dimethyl diallyl ammonium chloride (DMDAAC), 0.2 gram Diethylene Glycol double methacrylate, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the initiator ammonium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash, then with 100 parts of natural rubbers, 30 parts of water-absorbing resin powders, 2.5 parts of sulphur, 1 part of promotor, 5 parts of zinc oxide, 2.5 part stearic acid, 20 parts of carbon blacks, 1 part of anti-aging agent carries out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 41 grams.
Embodiment 5
With 2.5 gram vinylformic acid, 3 gram sodium acrylates, 3.5 gram acrylamide, 1 gram dimethyl diallyl ammonium chloride (DMDAAC), 0.4 Diethylene Glycol double methacrylate, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the initiator ammonium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of ethylene-propylene rubber(EPR), 30 parts of water-absorbing resin powders, 5 parts of zinc oxide, 1 part of stearic acid, 2 parts of promotor, 1.5 part sulphur, 20 parts of carbon blacks carry out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 43 grams.
Embodiment 6
With 2 gram vinylformic acid, 3 gram sodium acrylates, 3 gram acrylamides, 2 gram 2-methylacryoyloxyethyl-dimethyl dodecyl bromination ammoniums (DMDA), 0.4 gram tetramethylolmethane double methacrylate, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the copolyreaction of initiator ammonium peroxydisulfate after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of ethylene-propylene rubber(EPR), 30 parts of water-absorbing resin powders, 5 parts of zinc oxide, 1 part of stearic acid, 2 parts of promotor, 1.5 part sulphur, 20 parts of carbon blacks carry out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 41 grams.
Embodiment 7
With 2.5 gram vinylformic acid, 3 gram sodium acrylates, 2 gram acrylamides, 2.5 gram 2-methylacryoyloxyethyl-dimethyl dodecyl bromination ammonium (DMDA), 0.3 gram ethylene glycol diacrylate, 50mL solvent hexanaphthene and 1 Ke Siban-60 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the initiator ammonium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of chloroprene rubbers, 30 parts of water-absorbing resin powders, 1 part of stearic acid, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 30 parts of potter's clay carry out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 43 grams.
Embodiment 8
With 2.5 gram vinylformic acid, 3 gram sodium acrylates, 3.5 gram acrylamide, 1 gram vinylformic acid stearyl alcohol ester, 0.4 Diethylene Glycol double methacrylate, 50mL solvent hexanaphthene and 1 gram tween-80 add in the reactor, be warming up to 75 ℃ under constantly stirring, drip the initiator ammonium persulfate copolyreaction after 4 hours, filter, the dry water-absorbing resin powder that gets of methanol wash is then with 100 parts of ethylene-propylene rubber(EPR), 30 parts of water-absorbing resin powders, 5 parts of zinc oxide, 1 part of stearic acid, 2 parts of promotor, 1.5 part sulphur, 20 parts of carbon blacks carry out blend in mill, vulcanize can water-swellable in 25 ℃ to 150 ℃ scopes rubber.Take by weighing these hydro-expansive rubber 8 grams and deionized water 80 grams, put into autoclave, sealing is warming up to 150 ℃ of insulations after 3 days with autoclave, reduces to room temperature rapidly, takes out sample, wipes the moisture on surface with filter paper, and weighing gets 43 grams.
Claims (8)
1, a kind of method for preparing high-temperature-rusistance water-expansible rubber, it is characterized in that with mass ratio being vinylformic acid, sodium acrylate, acrylamide, heat resist modification monomer and the linking agent of 20-40: 30-60: 10-50: 10-60: 0.1-10, add in the reactor with solvent and dispersion agent, stir the back of heating up and drip the initiator copolyreaction, refilter, methanol wash dry the water-absorbing resin powder, the blend in mill with rubber and water-absorbing resin powder then, add vulcanizing ingredient vulcanize high-temperature-rusistance water-expansible rubber.
2, a kind of method for preparing high-temperature-rusistance water-expansible rubber according to claim 1 is characterized in that the heat resist modification monomer is a vinyl-acetic ester, butyl acrylate, Octyl acrylate, vinylformic acid lauryl alcohol ester, vinylformic acid stearyl alcohol ester, butyl methacrylate, Octyl methacrylate, methacrylic acid lauryl alcohol ester, methacrylic acid stearyl alcohol ester, 2-acrylamido-2-methyl propane sulfonic acid, 3-acrylamido oxypropyl trimethyl ammonium chloride, methacryloyl amido oxypropyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride or 2-methylacryoyloxyethyl-dimethyl dodecyl bromination ammonium.
3, a kind of method for preparing high-temperature-rusistance water-expansible rubber according to claim 1, it is characterized in that linking agent is ethylene glycol diacrylate, Diethylene Glycol double methacrylate, polyoxyethylene glycol double methacrylate, N, N '-methylene-bisacrylamide, tetramethylolmethane double methacrylate or Vinylstyrene.
4, a kind of method for preparing high-temperature-rusistance water-expansible rubber according to claim 1 is characterized in that solvent is toluene, dimethylbenzene and hexanaphthene.
5, a kind of method for preparing high-temperature-rusistance water-expansible rubber according to claim 1 is characterized in that dispersion agent is span-80, Si Ban-60, Si Ban-20, tween-80, Tween-60, tween 20, Sodium dodecylbenzene sulfonate.
6, a kind of method for preparing high-temperature-rusistance water-expansible rubber according to claim 1 is characterized in that rubber is natural rubber, chloroprene rubber, ethylene-propylene rubber(EPR), paracril, chlorinatedpolyethylene, urethanes, viton, silicon rubber, isoprene-isobutylene rubber or styrene-butadiene rubber(SBR).
7, the method for preparing hydro-expansive rubber according to claim 1, the granularity that it is characterized in that the water-absorbing resin powder is less than 5 μ m.
8, the method for preparing hydro-expansive rubber according to claim 1 is characterized in that initiator is Potassium Persulphate or ammonium persulphate.
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| CNB2005100199726A CN1331936C (en) | 2005-12-08 | 2005-12-08 | Method for preparing high-temperature-rusistance water-expansible rubber |
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| CNB2005100199726A CN1331936C (en) | 2005-12-08 | 2005-12-08 | Method for preparing high-temperature-rusistance water-expansible rubber |
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| CN101967240A (en) * | 2010-09-21 | 2011-02-09 | 重庆市万通工业有限公司 | Water swelling rubber, metallic composite sealing material and preparation methods thereof |
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| CN103570985A (en) * | 2013-10-09 | 2014-02-12 | 中国石油化工股份有限公司 | Water-swelling rubber composite material, and preparation method and application thereof |
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| JPH07100786B2 (en) * | 1986-05-30 | 1995-11-01 | シ−アイ化成株式会社 | Water-swellable waterproof composition |
| JP2592567B2 (en) * | 1992-06-19 | 1997-03-19 | シーアイ化成株式会社 | Water swellable rubber |
| CZ70097A3 (en) * | 1997-03-07 | 1998-09-16 | Jiří Ing. Šulc | Composite water-swelling elastomers and process for preparing thereof |
| DE19800489A1 (en) * | 1998-01-09 | 1999-07-15 | Thomas Prof Dr Mang | Polysaccharide-containing sealing composition |
| JP4103108B2 (en) * | 2002-06-11 | 2008-06-18 | 東洋ゴム工業株式会社 | Rubber composition for tire tread |
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| CN101963051A (en) * | 2010-02-08 | 2011-02-02 | 张宏亮 | Oil well packer |
| CN101967240A (en) * | 2010-09-21 | 2011-02-09 | 重庆市万通工业有限公司 | Water swelling rubber, metallic composite sealing material and preparation methods thereof |
| CN101974193A (en) * | 2010-11-17 | 2011-02-16 | 武汉工程大学 | Method for preparing low-leaching-rate water-swellable rubbers |
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| CN103570985A (en) * | 2013-10-09 | 2014-02-12 | 中国石油化工股份有限公司 | Water-swelling rubber composite material, and preparation method and application thereof |
| CN103554333A (en) * | 2013-11-19 | 2014-02-05 | 宜兴丹森科技有限公司 | Preparation method of high strength super absorbent resin |
| CN106084347A (en) * | 2016-06-23 | 2016-11-09 | 安徽荣达阀门有限公司 | A kind of low temperature resistant water-swellable water proof rubber encapsulant and preparation method thereof |
| CN107641274A (en) * | 2017-09-30 | 2018-01-30 | 咸阳橡胶工业制品研究所有限公司 | Type high-temperature-rusistance water-expansible rubber composite seal and preparation method during one kind control |
| CN109354734A (en) * | 2018-10-25 | 2019-02-19 | 西北橡胶塑料研究设计院有限公司 | A kind of flame retardant type hydro-expansive rubber material and preparation method thereof |
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